Charge dissipation modifiers for olefinic interpolymer compositions

ABSTRACT

Olefinic interpolymer compositions comprising the olefinic interpolymer, residuals from a transition metal catalyst and boron containing activator package, and a charge dissipation modifier and methods for making them. The compositions have dissipation factors that are at least 50% less than the corresponding olefinic interpolymer compositions which have not been treated with charge dissipation modifiers. The compositions are useful in wire and cable applications.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation application of U.S. application Ser.No. 10/691,163, filed Oct. 22, 2003, now U.S. Pat. No. 7,144,934, whichclaims the benefit of U.S. Provisional Application No. 60/420,879, filedOct. 24, 2002, incorporated herein by reference.

FIELD OF THE INVENTION

The present invention relates to olefinic interpolymer compositionscomprising an olefinic interpolymer, post-reactor residuals of atransition metal catalyst and a boron containing activator package, anda charge dissipation modifier. In another aspect, this invention relatesto a process for lowering the dissipation factor of olefinicinterpolymer compositions prepared with a transition metal catalyst incombination with a boron containing activator package, by addition of acharge dissipation modifier to the interpolymer composition. In yetanother aspect, the invention relates to wire and cable (W&C) productscontaining these olefinic interpolymer compositions.

BACKGROUND OF THE INVENTION

The discovery of transition metal catalysts, especially metallocene andconstrained geometry catalysts, for the preparation of olefinicinterpolymers has resulted in the synthesis of a wide range of new anduseful olefinic interpolymer compositions. These transition metalcatalysts are typically activated with boron containing activatorpackages. Following polymer formation, the catalyst-activator systemsare deactivated by addition of water, methanol, or other catalystdeactivation agents. After isolation, the resulting olefinicinterpolymer compositions retain residuals of the catalyst-activatorsystems and typically have dissipation factors greater than 0.10. Adissipation factor as low as possible is desired for olefinicinterpolymer compositions in electrical applications. The olefinicinterpolymer compositions can be acid washed or steam stripped to removeor reduce catalyst and activator residuals which further can lower thedissipation factor of the olefinic interpolymer composition to 0.01 orless depending on how the composition is washed or steam stripped. U.S.Pat. No. 3,819,591 provides examples of acid washing techniques and U.S.Pat. No. 3,076,795 and U.S. Pat. No. 3,590,026 provide examples of steamstripping techniques. While these techniques may effectively lower thedissipation factor, acid washing and steam stripping add an additionalstep and additional manufacturing costs to the preparation of theolefinic interpolymer compositions and are environmentally undesirableas each creates an additional waste stream, which must be disposed.

It has now been surprisingly discovered that by adding specific chargedissipation modifiers to olefinic interpolymer compositions preparedwith transition metal catalysts and boron containing activator packages,the dissipation factors can be lowered to levels which are at leastabout 50% less than dissipation factors of the corresponding olefinicinterpolymer compositions which have not been treated with the chargedissipation modifiers, thus providing simpler, lower cost, moreenvironmentally friendly olefinic interpolymer compositions forelectrical applications, particularly low and medium voltage wire andcable insulation and jacketing.

SUMMARY OF THE INVENTION

One aspect of this invention is an olefinic interpolymer compositioncomprising an olefinic interpolymer, post-reactor residuals of atransition metal catalyst and a boron containing activator package, anda charge dissipation modifier, the composition having a dissipationfactor which is at least about 50% lower than the same olefinicinterpolymer composition not containing a charge dissipation modifier ofthis invention, the charge dissipation modifier being selected from:

-   -   a) amine compounds of the formula (I) an (II):

-   -    wherein x is 3 and each R is independently selected from        linear, branched and cyclic hydrocarbyl groups and hydrogen or        together two or more R substituents are a cyclic hydrocarbyl        group and each R₁₋₅ is independently selected from linear,        branched and cyclic hydrocarbyl groups and hydrogen or together        two or more of the R₁₋₅ substituents are a cyclic hydrocarbyl        group;    -   b) silica compounds; and    -   c) phosphoric acid and mixtures thereof.

Another aspect of this invention is a process for improving theelectrical properties of an olefinic interpolymer composition preparedwith a transition metal catalyst and boron containing activator package,by adding a charge dissipation modifier to the olefinic interpolymercomposition. The charge dissipation modifier can be added to a solutionpolymerization process as soon as the desired level of polymerization isattained. Thus, the charge dissipation modifier can be added to anolefinic interpolymer composition-solvent solution after the solutionexits the reactor in a continuous solution process or if a solutionbatch process is being used, added directly into the reactor vesselafter the polymerization has reached the desired level of completion oradded to the solution after it has been removed from the reactor.Additionally, the charge dissipation modifier can be added to a solidolefinic interpolymer composition which has been prepared by a slurry orgas phase process and isolated. The charge dissipation modifier is addedusing methods known in the art to intimately mix the olefinicinterpolymer composition and the charge dissipation modifier.

Yet another aspect of the invention is a wire and cable productcontaining an olefinic interpolymer composition of this invention.

DESCRIPTION OF THE PREFERRED EMBODIMENTS

The olefinic interpolymer compositions which show improved dissipationfactors after addition of a charge dissipation modifier of the inventionare prepared in a polymerization process which employs a transitionmetal catalyst and a boron containing activator package. In general,such polymerizations may be conducted in a solution, slurry, or gasphase process and under conditions well known in the art forZiegler-Natta or Kaminsky-Sinn type polymerization reactions, that is,temperatures from 0–250° C., preferably 30 to 200° C., and pressuresfrom atmospheric to 10,000 atmospheres.

The olefinic interpolymers are prepared from at least one C₂₋₂₀ α-olefinmonomer and optionally, at least one polyene monomer. The α-olefin maybe an aliphatic, an aromatic or a cyclic compound, such as cyclobutene,cyclopentene, or norbornene, including norbornene substituted in the 5and 6 position with C₁₋₂₀ hydrocarbyl groups. The α-olefin is preferablya C₂₋₂₀ aliphatic compound, more preferably a C₂₋₁₆ aliphatic compound.Preferred α-olefin monomers include 4-vinylcyclohexene,vinylcyclohexane, norbornadiene and C₂₋₁₀ aliphatic α-olefins(especially ethylene, propylene, isobutylene, butene-1, pentene-1,hexene-1,3-methyl-l-pentene, 4-methyl-l-pentene, octene-1, decene-1,dodecene-1 and styrene), and mixtures thereof. Most preferred monomersare ethylene, and mixtures of ethylene with at least one of propylene,4-methyl-l-pentene, butene-1, hexene-1, octene-1 and styrene.

The polyene monomer, if employed, can be either a crosslinking site or abranching site or both. Each polyene monomer is desirably a C₄₋₄₀ dienemonomer (also referred to herein as a “diolefin”) and more desirably isa nonconjugated diolefin. The nonconjugated diolefin can be a C₆₋₁₅straight chain, branched chain or cyclic hydrocarbon diene. Illustrativenonconjugated dienes are straight chain acyclic dienes such as1,4-hexadiene, 1,5-heptadiene, and 1,6-octadiene; branched chain acyclicdienes such as 5-methyl-1,4-hexadiene, 2-methyl-1,5-hexadiene,6-methyl-1,5-heptadiene, 7-methyl-1,6-octadiene,3,7-dimethyl-1,6-octadiene, 3,7-dimethyl-1,7-octadiene,5,7-dimethyl-1,7-octadiene, 1,7-octadiene, 1,9-decadiene and mixedisomers of dihydromyrcene; single ring alicyclic dienes such as1,4-cyclohexadiene, 1,5-cyclooctadiene and 1,5-cyclododecadiene;multi-ring alicyclic fused and bridged ring dienes such astetrahydroindene, methyl tetrahydroindene, dicyclopentadiene,bicyclo-(2,2,1)-hepta-2,5-diene (norbornadiene), methyl norbornadiene;alkenyl, alkylidene, cycloalkenyl and cycloalkylidene norbornenes suchas 5-methylene-2-norbornene (MNB), 5-ethylidiene-2-norbornene (ENB),5-vinyl-2-norbornene (VNB), 5-propenyl-2-norbornene,5-isopropylidene-2-norbornene, 5-(4-cyclopentenyl)-2-norbornene and5-cyclohexylidene-2-norbornene.

When the diolefin is a conjugated diene, it can be 1,3-pentadiene,1,3-butadiene, 2-methyl-1,3-butadiene, 4-methyl-1,3-pentadiene, or1,3-cyclopentadiene. The diene is preferably a nonconjugated dieneselected from ENB, 1,4-hexadiene and norbornadiene, more preferably,ENB.

Examples of transition metal catalysts which, in combination with boroncontaining activator packages, typically produce olefinic interpolymercompositions with dissipation factors greater than 0.10 are listed in WO98/49212, U.S. Pat. No. 5,965,756, U.S. Pat. No. 6,160,066, U.S. Pat.No. 6,143,682, WO 00/02891, WO 00/02891, and U.S. Pat. No. 6,127,497(late transition metal catalysts), the contents of which areincorporated by reference. These catalysts can be used separately or incombination (dual catalyst systems) and in continuous or batch reactorprocesses employing single or multiple reactors.

The transition metal catalysts are rendered catalytically active by aboron containing activator package. The activator package contains aboron compound and optionally, an aluminum compound. Examples of boroncompounds which can be used in the activator package include, but arenot limited to, fluorinated tri(hydrocarbyl)boron compounds (includingperfluorinated derivatives thereof) having from 1 to 10 carbon atoms ineach hydrocarbyl or fluorinated hydrocarbyl group. Perfluorinatedtri(aryl)boron compounds are preferred. Most preferred istris(pentafluorophenyl)borane (hereinafter “FAB”). As mentioned above,these boron compounds can be used as the sole component of the activatorpackage or preferably, they can be used in combination with an aluminumcompound. Examples of an aluminum compound include, but are not limitedto, a trialkyl aluminum compound having from 1 to 4 carbon atoms in eachalkyl group or a polymeric or oligomeric alumoxane. A preferredactivator package combines a fluorinated tri(hydrocarbyl)boron compoundhaving from 1 to 20 carbon atoms in each hydrocarbyl group, mostpreferably FAB, with a trialkyl aluminum compound having from 1 to 4carbon atoms in each alkyl group. Another preferred activator packagecombines FAB and triisobutyl aluminum modified methylalumoxane (MMAO).Both preferred activator packages are combinations which are efficientat producing olefinic interpolymers used in this invention but theresulting olefinic interpolymer compositions typically have dissipationfactors greater than 0.10.

Borates are not boron compounds used in the activator packages of thisinvention and are not boron species of this invention.

When these transition metal catalysts and activator packages are used ina solution process to prepare olefinic interpolymer compositions,suitable inert solvents for these solution polymerizations include, forexample, straight and branched-chain hydrocarbons such as isobutane,butane, pentane, hexane, heptane, octane, as well as mixtures of alkanesincluding kerosene and isoparafins, cyclic and alicyclic hydrocarbonssuch as cyclohexane, cycloheptane, methylcyclohexane,methylcycloheptane, and mixtures thereof; and aromatic andalkyl-substituted aromatic compounds such as benzene, toluene, xylene,and ethylbenzene. Suitable solvents also include liquid olefins that mayact as monomers or comonomers including butadiene, cyclopentene,1-hexene, 4-vinylcyclohexene, vinylcyclohexane, 3-methyl-l-pentene,4-methyl-l-pentene, 1,4-hexadiene, 1-octene, 1-decene, styrene,divinylbenzene, allylbenzene, and vinyltoluene (including all isomersalone or in a mixture). Mixtures of the foregoing are also suitable. Ifdesired, normally gaseous olefins can be converted to liquids byapplication of pressure and used as inert liquids.

Adding charge dissipation modifiers of this invention to olefinicinterpolymer compositions prepared with transition metal catalysts andboron containing activator packages can lower the dissipation factor byat least about 50% compared to the same olefinic interpolymercompositions which have not been treated with charge dissipationmodifiers of this invention. Preferably, a sufficient amount of chargedissipation modifier of this invention is added to the olefinicinterpolymer composition to lower the dissipation factor to less than0.12, preferably less than 0.10, more preferably less than 0.05, andmost preferably less than 0.01 without post-treatment of the olefinicinterpolymer composition by acid washing or steam stripping.

Although not wishing to be bound by any particular theory, it isbelieved that in order for the charge dissipation modifier to functionproperly, it must be able to physically interact with or contact theactivator/catalyst residuals from the polymerization reaction to form anolefinic interpolymer composition having a dissipation factor about 50%less than the corresponding untreated olefinic interpolymer composition.Such an interaction can only take place if the olefinic interpolymercomposition and the charge dissipation modifier are intimately mixed,for example, in solution or in the melt state.

A preferred method for adding the charge dissipation modifier to theolefinic interpolymer composition is to add the charge dissipationmodifier to an olefinic interpolymer composition-solvent solutionresulting from a solution polymerization process.

When the charge dissipation modifier is added to an olefinicinterpolymer composition-solvent solution, it has the ability tofunction both as a deactivation agent and a charge dissipation modifier.When the charge dissipation modifier is also the deactivation agent, noadditional deactivation agent need be added to the olefinic interpolymercomposition-solvent solution. However, a separate deactivation agentsuch as water or methanol is typically added to the solution incombination with a charge dissipation modifier. The charge dissipationmodifier can be used in both continuous and batch reactor processes andin processes using single or multiple reactors in series or parallel.Whether added as a combination deactivation agent and charge dissipationmodifier or solely as a charge dissipation modifier in a continuousprocess, the charge dissipation modifier is preferably added to the exitstream from the reactor.

When used in a single reactor continuous process and as either acombination deactivation agent/charge dissipation modifier or solely asa charge dissipation modifier, the charge dissipation modifier ispreferably added to the interpolymer composition-solvent solution at anypoint after the solution leaves the reactor and the interpolymercomposition is still in solution. If employing a dual reactor ormultiple reactor continuous process in series, the charge dissipationmodifier is preferably added after the interpolymer composition-solventsolution leaves the last reactor and the interpolymer composition isstill in solution. If the continuous process is a multiple reactorparallel process, the charge dissipation modifier can be added after thesolution leaves each reactor or after all the reactor exit streams arecombined. In a batch solution process, the charge dissipation modifieris preferably added to the reaction vessel when the reaction has reachedits desired level of completion.

When a separate deactivation agent is used, the deactivation agent canbe added in combination with the charge dissipation modifier at the samepoint as the charge dissipation modifier, before the charge dissipationmodifier is added to the interpolymer composition-solvent solution, orafter the charge dissipation modifier is added to the interpolymercomposition-solvent solution as long as the polymerization reaction hasreached the desired level of completion and preferably before thesolvent is removed from the olefinic interpolymer composition-solventsolution.

When a separate deactivation agent is added to the olefinic interpolymercomposition, the dissipation factor is typically greater than about0.10. Levels below about 0.10 are not typically obtained by use ofdeactivation agents such as water and methanol.

It should be noted that in general, the higher the efficiency of thetransition metal catalyst and activator package, the lower thedissipation factor of the resulting olefinic interpolymer. In situationsof high catalyst/activator efficiency (e.g., efficiencies of 10 milliongrams polymer/gram transition metal and greater), addition of a chargedissipation modifier may not be necessary for the material to be used insome electrical applications. However, if a charge dissipation modifieris used, the dissipation factor will most likely be improved, but theimprovement may not approach the 50% level.

Another method for adding the charge dissipation modifier to theolefinic interpolymer composition is to add a charge dissipationmodifier to the olefinic interpolymer composition after it has beenisolated as a solid from a solution, slurry, or gas phase process. Whenthis method of charge dissipation modifier addition is employed, theolefinic interpolymer composition and charge dissipation modifier mustbe intimately mixed together so that the charge dissipation modifier andthe catalyst/activator residuals come into sufficient physical contactwith each other to lower the interpolymer composition dissipation factorby at least about 50%. Examples of methods to accomplish this include,but are not limited to, melt blending the olefinic interpolymer with thecharge dissipation modifier in an extruder or other melt blendingapparatus or redissolving the olefinic interpolymer in a suitablesolvent and treating the solution containing the olefinic interpolymerwith a charge dissipation modifier.

Yet, another method for adding the charge dissipation modifier to anolefinic interpolymer compositions is to blend an olefinic interpolymercomposition which has been treated with an excess of charge dissipationmodifier with an olefinic interpolymer composition which has not beentreated with a charge dissipation modifier. The compositions can beblended by known methods in the art such as melt blending in anextruder.

Charge dissipation modifiers which, when added to olefinic interpolymercompositions, lower the dissipation factor of the compositions by atleast about 50% include:

-   -   a) amine compounds of the formula (I) and (II):

-   -   wherein x is 3 and each R is independently selected from linear,        branched and cyclic hydrocarbyl groups and hydrogen or together        two or more R substituents are a cyclic hydrocarbyl group and        each R₁₋₅ is independently selected from linear, branched and        cyclic hydrocarbyl groups and hydrogen or together two or more        of the R₁₋₅ substituents are a cyclic hydrocarbyl group;    -   b) silica compounds; and    -   c) phosphoric acid and mixtures thereof.

The amine compounds used as charge dissipation modifiers in thisinvention can be any primary amine, secondary amine, tertiary amine, orammonia. The R and R₁₋₅ groups can be any hydrocarbyl group such aslinear, branched, or cyclic aliphatic or aromatic compounds, preferablya C₁–C₅₀ aliphatic compound, more preferably a C₃–C₂₀ aliphaticcompound. Examples of amine compounds include aniline, isopropylamine,ammonia, pyridine, and most preferably N, N-octadecyl methyl amine (alsoreferred to herein as “bis-tallowalkyl methyl amine”).

The silica compounds used as charge dissipation modifiers in thisinvention include SiO₂ in any form. Preferred are surface modifiedsilica and high surface area silica. Most preferred is hydrophobicsilica.

The amount of charge dissipation modifier added to the olefinicinterpolymer composition can be determined by the amount of transitionmetal catalyst or by the amount of boron containing compound used toprepare the interpolymer. The lower the catalyst efficiency, the greaterthe amount of catalyst needed to prepare a given quantity ofinterpolymer and the more charge dissipation modifier needed to lowerthe dissipation factor of the interpolymer composition by at least about50%. Preferably, the amount of charge dissipation modifier added issufficient to reduce the dissipation factor to less than 0.12, morepreferably less than 0.10. For purposes of this invention, the amount ofmetal atom from the transition metal catalyst in the interpolymercomposition is used to determine the amount of charge dissipationmodifier needed. Preferably, the transition metal atom (titanium,zirconium and hafnium for example) to charge dissipation modifier ratiois at least 1:1000, more preferably at least 1:100, and most preferablyat least 1:10.

The physical properties such as melting point, glass transitiontemperature, and molecular weight distribution of olefinic interpolymersprepared with transition metal catalyst and boron containing activatorpackages do not appear to be affected by addition of the chargedissipation modifier(s) of this invention. Olefinic interpolymercompositions, which have been treated with charge dissipationmodifier(s) of this invention, have dissipation factors sufficiently lowfor use in most wire and cable insulation and jacketing applications.For most low voltage applications a dissipation factor less than orequal to about 0.10 is required. For medium voltage applications, adissipation factor less than or equal to about 0.01 is required. Thesedissipation factors are not absolute and the determining factor inwhether or not a particular product can be used in low and mediumvoltage wire and cable insulation and jacketing is whether or not theproduct passes long term underwater testing. Typically, products whichdo not have dissipation factors less than about 0.10 fail such tests.

The following examples illustrate but do not, either explicitly or byimplication, limit the present invention. Unless otherwise stated, allparts and percentages are by weight, on a total weight basis. Numericranges include the end points unless stated otherwise. Examples of thepresent invention are identified by Arabic numerals and comparativeexamples are represented by letters of the alphabet.

EXAMPLES

Except as specifically stated below, the continuous polymerizationprocess as described in WO 98/49212 for the preparation of Examples 4–7was used to prepare the olefinic interpolymer composition-solventsolutions used in the Examples of this invention and the ComparativeExamples. The process was designed for continuous addition of reactantsand continuous removal of polymer solution, devolatilization of solventand unreacted monomers, and polymer recovery. Ethylene, propylene andENB monomers, titanium[N-(1,1-dimethylethyl)-1,1-dimethyl-1-(1,2,3,3a,8a-eta)-1,5,6,7-tetrahydro-2-methyl-s-indacen-1-yl]silanaminato(2-)-.kappa.N][(1,2,3,4-eta)-1,3-pentadienecatalyst (also referred to as(t-butylamido)dimethyl(5–2-methyl-s-indacen-1-yl)silane titanium (II)1,3-pentadiene catalyst), a boron containing activator packageconsisting of a combination of FAB and MMAO, and Isopar-E solvent werecontinuously added and/or recycled to a single reactor.

In the Examples, charge dissipation modifier solutions were preparedwith an lsopar-E solvent and introduced into the hot olefinicinterpolymer composition-solvent solution after the solution exited thereactor. The concentration of the charge dissipation modifier solutionwas adjusted manually, based on catalyst efficiency, to maintain atitanium metal to charge dissipation modifier molar ratio of 1:1000. Theolefinic interpolymer composition-solvent solution flow was maintainedfor at least two hours prior to collection of the interpolymercomposition. The olefinic interpolymer composition-solvent solutioncontaining the charge dissipation modifier was pumped through a staticmixer and a post-reactor heater. The post-reactor heater temperature wasmaintained at 150° C. The interpolymer composition was pumped into aseparator, where unreacted comonomers, unreacted hydrogen, unreactedENB, and solvent were volatilized, yielding a molten interpolymercomposition comprising an ethylene/propylene/diene interpolymer(“EPDM”), the charge dissipation modifier and residuals of catalyst andactivator. After collection of the interpolymer composition wascomplete, charge dissipation modifier solution flow was shut off, andthe system purged with untreated interpolymer composition for at leasttwo hours to clear the separator of any material that had been treatedby a charge dissipation modifier. The charge dissipation modifieradditive tank was flushed with fresh solvent prior to adding the newcharge dissipation modifier solution to prevent cross contamination ofthe charge dissipation modifier. After collection, the interpolymercomposition was dried at 115° C. in a vacuum oven for at least 8 hoursto ensure complete solvent devolatilization.

Except as specifically explained later, compositions of the ComparativeExamples were made in the same way as described in the precedingparagraph except deactivation agents were added in place of the chargedissipation modifiers. The deactivation agents in the ComparativeExamples were used as received and without further purification. Waterand methanol were purchased from Fisher Scientific International Inc.PEP-Q was obtained from Clariant Corp. Tripropylphosphate and phosphoricacid were obtained from Aldrich Chemical Company (now Sigma-AldrichCompany). Silica (AEROSIL® R 972, a fumed hydrophobic silica) wasobtained from Degussa Corp. Bis-tallowalkyl methyl amine (Armeen M2HT)was obtained from Akzo Nobel Inc.

The dried olefinic interpolymer composition was prepared for electricaltesting in both the Examples and Comparative Examples by blending 50 gof interpolymer composition in a Haake mixer equipped with cam mixingblades at 100° C. with 1 g of dicumyl peroxide, using a mixing speed of55 rpm for 3 minutes. 12 grams of the interpolymer composition/peroxideblend were pressed between two Mylar® polyester sheets (DuPont Company)in a mold to prepare plaques that were 3.5″ diameter and approximately0.17 cm thickness. The plaques were crosslinked by pre-heating the pressand mold at 375° F. (191° C.) for at least 3 minutes. The molds wereloaded with interpolymer composition, pressed in a Tetrahedron Press to20 tons of pressure for 3 minutes, cooled to 120° F. (49° C.) using 240as the press rate setting, and maintained under these conditions for 3minutes. Crosslinked 3.5″ diameter plaques of approximately 0.17 cmthickness were obtained.

The dissipation factor of the plaques was measured according to ASTMD150 at 130° C. using a Tettex Model 2914 Test Cell for Solid Insulants.A Tettex Model 5283 Power Transformer supplied the voltage to the TestCell. A Tettex Model 2966 Temperature Control Unit heated the Test Cellelectrodes. Resistance was measured on the Tettex Model 5476A ResistanceBridge. (Tettex equipment from Tettex Corporation).

Examples 1–3 and Comparative Examples A–H

EPDM-1, an interpolymer composition having 70 wt % ethylene, 29.5 wt %propylene, 0.5 wt % ENB, a Mooney viscosity of 40 and 1.3 million grams(MM g) interpolymer/g titanium, was prepared. This composition wasemployed in Examples 1–3 and Comparative Examples A–G. In Example 1–3,various charge dissipation modifiers were added. In Comparative ExampleA, neither a charge dissipation modifier nor a deactivation agent wasadded. In Comparative Examples B–G, various deactivation agents wereadded. The dissipation factor of each was measured. Table 1 shows thetype and amount of charge dissipation modifier (Examples) anddeactivation agent (Comparative Examples) and the dissipation factor foreach composition. Comparative Example H, which utilized EPDM-A is alsoincluded in this Table. EPDM-A was Nordel® 2722E (DuPont Dow ElastomersLLC), an EPDM composition commercially used in electrical applicationswhich had 72 wt % ethylene, 23.6 wt % propylene, 4.4 wt % ENB, a Mooneyviscosity of 27 and was produced with a conventional Ziegler-Nattacatalyst and steam stripped. Charge dissipation modifier is designated“CDM” and deactivation agent is designated “DEA” in this Table and somelater Tables as well.

TABLE 1 Ex. Concentration and CDM/DEA g Dissi- Comp. Interpolymer per8000 ml pation Ex. Composition CDM/DEA Solvent⁵ Factor Ex. 1 EPDM-1Bis-tallowalkyl 48.8 g 0.031 methyl amine Ex. 2 EPDM-1 Silica  5.5 g0.021 Ex. 3 EPDM-1 Phosphoric Acid  8.9 g 0.061 Comp. EPDM-1 None —0.454 Ex. A Comp. EPDM-1 Water  1.6 g 0.125 Ex. B Comp. EPDM-1 IRGANOX ®1010³ 2.88 g/0.18 g 0.156 Ex. C and Water Comp. EPDM-1 PEP-Q⁴ 94.2 g0.341 Ex. D Comp. EPDM-1 Stearic Acid 25.2 g 0.195 Ex. E Comp. EPDM-1Methanol  2.9 g 0.149 Ex. F Comp. EPDM-1 Tripropylphosphate 19.3 g 0.334Ex. G Comp. EPDM-A — — 0.003 Ex. H ³Pentaerythriol Terakis(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate) from Ciba SpecialtyChemicals Corp. ⁴Tetrakis(2,4-di-tert-butylphenyl)-4,4-biphenylenediphosphonite ⁵Values for a 454 g polymer/hr production rate, 1.3 MM gpolymer/g Ti catalyst efficiency, and 8 g/minute modifier solution flowrate.

All of Comparative Examples A–G, including those treated with adeactivation agent, had higher dissipation factors than the commerciallyutilized composition and control, EPDM-A of Comp. Ex. H, which had beensteam stripped. Comparative Example A, made with no deactivation agent,had the highest dissipation factor (0.454) of all the testedinterpolymer compositions. When water was used as a deactivation agent(Comp. Ex. B), the dissipation factor was reduced from 0.454 to 0.125.Similarly, when methanol was used as the deactivation agent (Comp. Ex.F), the dissipation factor was reduced to 0.149. Thus, water andmethanol are each somewhat effective at reducing the dissipation factorof the olefinic interpolymer composition. However, the dissipationfactors of these Comparative Examples are still an order of magnitudetoo high for the compositions to be used in most electricalapplications.

IRGANOX® 1010 and water were added as the deactivation agent in Comp.Ex. C and and PEP-Q was the deactivation agent in Comp. Ex. D. Thesedeactivation agents are commonly used as additives and stabilizersagainst polymer decomposition. IRGANOX® 1010 is not a charge dissipationmodifier of the invention. PEP-Q is a functionalized molecule containingphosphorus but also is not a charge dissipation modifier of theinvention. As shown in Table 1, Comp. Ex. D had a dissipation factor of0.341. Comp. Ex. C had a lower dissipation factor, 0.156. The lowerdissipation factor of Comp. Ex. C is thought to be due mainly to theeffect of the water. Again, these additives failed to reduce thedissipation factor of the interpolymer compositions to desirable levelsbelow 0.10.

As in Comp. Ex. D, the deactivation agent used in Comp. Ex. G containeda phosphorus atom, but is not a charge dissipation modifier of theinvention. Comp. Ex. G gave a fairly high dissipation factor (0.334),similar to the dissipation factor measured for Comp. Ex. D. Thedeactivation agents of both Comp. Exs. D and G contain phosphorus butare chemically different than phosphoric acid (Ex. 3) which is a chargedissipation modifier of the invention.

Comparative Example E had a dissipation factor of 0.195. Thedeactivation agent in this comparative example was stearic acid, whichcontains an acid functionality but failed to reduce the dissipationfactor of the olefinic interpolymer composition to levels desirable foruse in most electrical applications.

Surprisingly, the interpolymer compositions of Examples 1–3, althoughtreated with charge dissipation modifiers that were quite different inchemical structure and composition, each had significantly improveddissipation factors relative to Comparative Examples A–G. As shown inTable 1, Examples 1–3 had dissipation factors of 0.031, 0.021, and0.061, respectively. These dissipation factors are almost an order ofmagnitude better than those obtained from Comparative Examples A–G. Inaddition, the dissipation factors of Ex. 1 and Ex. 2 represent a 93–95%reduction and Ex. 3 an 87% reduction in dissipation factor compared tothe untreated interpolymer composition (Comp. Ex. A). Further, thedissipation factors of these three Examples represent a 51–83% reductionin dissipation factor compared to water treated interpolymer compositionof Comp. Ex. B. Although Examples 1–3 did not have dissipation factorsas low as that of Comp. Ex. H, the dissipation factors of the Examplesare low enough to meet the electrical requirements for most low voltageapplications without the disadvantage of the additional steps of steamstripping and disposing of the steam stripping waste stream that areassociated with Comp. Ex. H.

Examples 4–8 and Comparative Example I

EPDM-2, an interpolymer composition having 70 wt % ethylene, 29.5 wt %propylene, 0.5 wt % ENB, a Mooney viscosity of 22 and 0.53 million grams(MM g) interpolymer/g titanium, was prepared using water as the catalystdeactivation agent. This composition was employed in Examples 4–8 andComparative Example I.

In Examples 4–8, various charge dissipation modifiers were blended withEPDM-2. Each charge dissipation modifier was blended with 50 grams ofEPDM-2 at a temperature of 70° C. and a mixing speed of 55 rpm for 5minutes in a Haake mixer equipped with cam mixing blades. Dicumylperoxide (1.0 g) was then added and the blend mixed for an additional 3minutes in the Haake mixer at 100° C. and a mixing speed of 55 rpm. Theblended samples were then pressed into plaques and cured according tothe procedure described above. The plaques were then tested at 130° C.according to ASTM D150. The type and amount of modifier added and theresulting dissipation factor of the blended examples is shown in Table2.

TABLE 2 Charge Amount of Example/ Interpolymer Dissipation CDM addedDissipation Comp. Ex. Composition Modifier (g) Factor Comp. EPDM-2 None— 0.068 Ex. I 4 EPDM-2 Aniline 0.261 0.009 5 EPDM-2 Pyridine 0.281 0.0026 EPDM-2 Isopropylamine 0.225 0.008 7 EPDM-2 25% ammonia 0.323 0.007 and75% water 8 EPDM-2 Bis-tallowalkyl 0.530 0.017 methyl amine

Examples 9 and 10 and Comparative Example J

EPDM-3, an interpolymer composition having 70 wt % ethylene, 29.5 wt %propylene, 0.5 wt % ENB, a Mooney viscosity of 22 and 0.56 million grams(MM g) interpolymer/g titanium, was prepared in the same way as EPDM-2except that, for Example 9, a charge dissipation modifier was added tothe interpolymer solution before the solvent was removed. The EPDM-3composition, absent the modifier, was employed in Comparative Example J.The interpolymer composition of Example 10 was prepared by blending 25grams of EPDM-3 with 25 grams of the Example 9 composition for 5 min.using a Haake mixer followed by treatment with peroxide and plaquepreparation. Results are shown in Table 3.

The dissipation factor of Ex. 9 was more than 50% less than that ofComp. Ex. J, the same composition but which had not been treated with acharge dissipation modifier. Further blending the composition of Ex. 9with equal parts of Comp. Ex. J reduced the dissipation factor by anorder of magnitude (Ex. 10). Thus, the dissipation factor of aninterpolymer composition can be reduced by sufficiently contacting itwith a composition containing excess charge dissipation modifier.

TABLE 3 Charge Amount of CDM Dissi- Example/ Interpolymer Dissipation inInterpolymer pation Comp. Ex. Composition Modifier Composition (g)Factor Comp. EPDM-3 None — 0.0629 Ex. J Ex. 9 EPDM-3 Bis-tallowalkyl0.989 0.0300 methyl amine Ex. 10 EPDM-3 Bis-tallowalkyl 0.49 0.0032methyl amine

Comparative Examples K and L

EPDM-4 was prepared by the process described above at the beginning ofthe Examples section except the boron containing activator package was acombination of N,N-bis(tallowalkyl)-N-methylammoniumtetrakis(2,3,4,5,6-pentafluorophenyl)borate (Boulder Scientific Company)and MMAO (Akzo-Nobel). The process yielded an interpolymer compositionhaving 70 wt % ethylene, 29.5 wt % propylene, 0.5 wt % ENB, a Mooneyviscosity of 20 and 2.14 MM g interpolymer/g titanium. This composition,EPDM-4, was employed in Comparative Examples K and L. In ComparativeExample L, EPDM-4 was blended with the charge dissipation modifier ofTable 4 and the dissipation factor measured.

As Table 4 shows, addition of a charge dissipation modifier of thisinvention to an EPDM prepared with borate activators is not effective inreducing the dissipation factor. In fact, the dissipation factorincreased.

TABLE 4 Charge Comp. Interpolymer Dissipation Amount of CDM DissipationEx. Composition Modifier added (g) Factor K EPDM-5 None — 0.093 L EPDM-5Bis-tallowalkyl 0.497 0.512 methyl amine

1. A method for making an olefinic interpolymer composition having a lowdissipation factor, said method comprising adding at least one chargedissipation modifier to an unmodified olefinic interpolymer composition,and wherein the unmodified olefinic interpolymer composition comprisingthe following: a) an olefinic interpolymer or a mixture of olefinicinterpolymers, each comprising at least one C₂–C₂₀ α-olefin monomer, andoptionally comprising at least one polyene, and b) post-polymerizationreactor residuals of at least one transition metal catalyst and a boroncontaining activator package; and wherein the at least one chargedissipation modifier is selected from the group consisting of: i) aminecompounds of the general formula (I) and (II):

 wherein x is 3, and each R is independently selected from linear,branched and cyclic hydrocarbyl groups and hydrogen, or together two ormore R substituents are a cyclic hydrocarbyl group, and each R₁₋₅ isindependently selected from linear, branched and cyclic hydrocarbylgroups and hydrogen, or together two or more of the R₁₋₅ substituentsare a cyclic hydrocarbyl group; ii) silica compounds; and iii)phosphoric acid; and iv) and mixtures thereof; and wherein the olefinicinterpolymer composition has a dissipation factor which is at least 50%lower than the dissipation factor of the unmodified olefinicinterpolymer composition.
 2. The method of claim 1, wherein the at leastone charge dissipation modifier is added to a solution comprising theunmodified olefinic interpolymer composition and a solvent.
 3. Themethod of claim 2, wherein the solution is formed from a solutionpolymerization process.
 4. The method of claim 3, wherein the solutionpolymerization process takes place in a continuous reactor processcomprising one or more reactors.
 5. The method of claim 4, wherein theat least one charge dissipation modifier is added to the solution, atany point after the solution leaves the last reactor, and when theunmodified olefinic interpolymer composition is still in solution. 6.The method of claim 3, wherein the solution polymerization process takesplace in a batch reactor process.
 7. The method of claim 6, wherein theat least one charge dissipation modifier is added to the reaction, afterthe reaction has reached its desired level of completion.
 8. The methodof claim 1, wherein the at least one charge dissipation modifier isadded, after the unmodified olefinic composition has been isolated, as asolid, from a solution, slurry or gas phase process.
 9. The method ofclaim 8, wherein the at least one charge dissipation modifier and theunmodified olefinic composition are mixed together using a melt blendingapparatus.
 10. The method of claim 1, wherein the at least one chargedissipation modifier is selected from the group consisting of aniline,isopropylamine, pyridine, and N,N-octadecyl methyl amine.
 11. The methodof claim 1, wherein the at least one charge dissipation modifier is asilica compound.
 12. The method of claim 1, wherein the at least onecharge dissipation modifier is phosphoric acid.
 13. The method of claim1, wherein the at least one C₂–C₂₀ α-olefin monomer is selected from thegroup consisting of ethylene, propylene, 1-butene, 1-hexene, 1-octene,and 4-methyl-1-pentene.
 14. The method of claim 1, wherein the at leastone olefinic interpolymer comprises two α-olefin monomers.
 15. Themethod of claim 14, wherein the α-olefin monomers are ethylene andoctene-1.
 16. The method of claim 1, wherein the α-olefin monomers areethylene and butene-1.
 17. The method of claim 1, wherein the unmodifiedolefinic interpolymer composition comprising a mixture of olefinicinterpolymers, each comprising two or three α-olefin monomers selectedfrom the group consisting of ethylene, propylene, butene-1 and octene-1.18. The method of claim 1, wherein the olefinic interpolymer comprisesat least one polyene.
 19. The method of claim 18, wherein the polyene isselected from the group consisting of 5-ethylidene-2-norbornene and5-vinyl-2-norbornene.
 20. The method of claim 1, wherein the olefinicinterpolymer composition has a dissipation factor of less than 0.12.